Hirschfeld-Klinger reaction shrinkage factor proving installation and method of testing thereof
Technical field
The present invention relates to a kind of device and method of surveying shrinkage factor, relate in particular to a kind of Hirschfeld-Klinger reaction shrinkage factor proving installation and method of testing thereof.
Background technology
Under certain pressure intensity, liquid crystalline solid, when its temperature is lower than fusing point slightly, particulate just will be arranged as stable structure regularly.Beginning is that the minority particulate is lined up according to certain rules, forms so-called nucleus, then grows into crystal grain one by one around these nucleus.Therefore, process of setting is exactly the process that produces nucleus and nucleus growth, and these two kinds of processes are carried out simultaneously.Temperature when liquid crystal solidifies is exactly a solidifying point, and temperature equals the fusing point of this crystal, but notion is different, and its solidifying point of crystals with different is also inequality.The liquid crystal material is emitted heat (be called heat of solidification, its numerical value equals melting heat) in process of setting, its temperature remains unchanged in process of setting, till liquid all becomes crystal.Non-crystal fluent meterial, in process of setting, the temperature reduction loses flowability gradually, becomes solid at last.It does not have certain solidifying point at process of setting, and is just corresponding with certain temperature range.
The characteristics of solidifying have determined goods in when casting, and in the phase transition process of solid, volume can change, and causes the physical dimension of goods to change, and breaks away from standard size by the liquid state of fusion; Also have, coating has been widely used for the protection of body surface, and coating solidifies after being applied to body surface, and volume will produce contraction in the process of solidifying; And shrink the formation possibly cause hole, make stress cracking, poor adhesive force; And then layering appears, warpage is so that coating comes off.Based on above reason, liquid becomes the problem that people are concerned about to the volumetric shrinkage in the solid process.
The contraction of goods has thermal shrinkage, and crystallization is shunk, oriented shrink, and compression is shunk, the negative contraction and post shrinkage.Wherein, thermal shrinkage is the contraction that the polymkeric substance of high temperature produces when cooling curing, be material intrinsic also be one of chief reason, show as linear shrinkage; Amount of contraction and material and the extraneous temperature difference also have the material coefficient of thermal expansion coefficient relevant.Crystallization is shunk and also can be called the phase transformation contraction, is meant the contraction that crystalline material is produced when when crystallization, just undergoing phase transition; During crystallization, macromolecular arrangement becomes closely orderly arrangement by random ball of string shape, and the volume of goods reduces.Amount of contraction is relevant with crystallinity, and the high more then shrinkage factor of crystallinity is big more.Oriented shrink is referring under the effect of mobile and shearing, can to produce molecular orientation to a certain degree, and during cooling curing, molecule has the trend that returns to the shape that curls, thereby on orientation, produces contraction; The shrinkage factor consistent with flow direction is called lateral shrinkage, is called vertical shrinkage factor perpendicular to the shrinkage factor of flow direction; Oriented shrink is relevant with the degree of orientation of molecule, and the high more then oriented shrink of degree of orientation is big more.Compression is shunk and is meant that under high pressure the specific volume of material changes, and at a certain temperature, high pressure makes the specific volume of material reduce, and the corresponding increase of density makes volume produce and shrinks.Negative contraction is a recovery of elasticity; Be meant when goods take out from mould, because the suddenly disappearing of die cavity internal pressure, the recovery of elasticity effect that the moulding material corresponding with compressibility has and the volumetric expansion phenomenon that produces; Product volume is shunk reduce, because therefore be called negative the contraction on the contrary with the contraction notion.Post shrinkage is that crystallization is incomplete when mould takes out at goods, takes out the continued crystallization again, knows that crystallization is complete, at this moment the contraction of the volume that produces.
The contraction of goods can be divided into three phases: phase one, the contraction (packing stage) before the gate solidification.In this stage, injected plastics material constantly injects in the mould, so depend primarily on the compensation ability of melt in the contraction in this stage.This process continues till gate solidification and the sealing always.The contraction in this stage and dwell pressure, the dwell time is relevant.Dwell pressure is big more, and the dwell time is long more, and shrinkage factor is more little.The contraction (cooling stage) of subordinate phase, goods cooling procedure in mould.From the whole process that is sealed to the demoulding, no longer include new melt and inject, crystallization this moment is shunk and is occupied an leading position, and the factor that therefore influences the crystallization contraction all can influence the contraction of goods.Phase III, the free shrink after the demoulding.Goods after the demoulding must at room temperature leave standstill a period of time, because the strand that has been orientated in the internal stress goods can relax, also be the process of the crystallization again of crystalline polymer this moment.Stress relaxation more greatly then takes place in freeze-oriented more easily, and then the contraction of goods is big more, and change in size is big more.The size of free shrink amount and goods, polymkeric substance thermal expansivity, the temperature of articles during demoulding, the temperature of external environment is relevant.
In the past, the method for surveying shrinkage factor was volume (or length of a certain direction) and the volume (or length of a certain direction) after the curing, the shrinkage from mold dimensions of measuring respectively before solidifying again.This method can't be observed the volume change in the solidification process.
Summary of the invention
To above-mentioned prior art, the present invention provides a kind of Hirschfeld-Klinger reaction shrinkage factor proving installation.Adopt proving installation of the present invention not only can detect phase one and the volumetric shrinkage of subordinate phase in the goods contraction process; Because the inner chamber at proving installation evenly is coated with release agent, can also detect the volumetric shrinkage of the phase III in the goods contraction process.Adopt proving installation of the present invention to carry out the test of Hirschfeld-Klinger reaction shrinkage factor and have the effect of instant tracking, can be used for measuring the shrinkage factor of any liquid when solidifying.
In order to solve the problems of the technologies described above; The technical scheme that a kind of Hirschfeld-Klinger reaction shrinkage factor of the present invention proving installation is achieved is: comprise housing; Said housing is made up of a cylindrical shell and the cast lid and the capping that are connected in said cylindrical shell two ends respectively, and the top of said cast lid is provided with the sprue gate that the cavity volume with said housing connects, and the sealing that is provided with flexible material in the said sprue gate is stifled; The junction that is positioned at the top in said cylindrical shell and said capping is provided with a mounting hole; The cavity volume of said mounting hole and said housing connects, be fitted with in the said mounting hole one have a volume markings glass tube, be provided with the sealing ring of flexible material between said mounting hole and the said glass tube.
Wherein, the cavity volume of said housing is a taper type cavity volume, and said cast lid is positioned at the little head end of said taper type cavity volume.Said mounting hole is a circular hole that is formed by the second semicircle vertical slot obvolvent on first semicircle vertical slot on the said capping end face and the said body end surface, and the bottom of the said first semicircle vertical slot is a platform.
Another technical scheme that a kind of Hirschfeld-Klinger reaction shrinkage factor of the present invention proving installation is achieved is: comprise housing, said housing is made up of the cylindrical shells of two axial butt joints, the cast lid that two are fixed on the cylindrical shell two ends after the butt joint respectively; The top of said cast lid is provided with the sprue gate that the cavity volume with said housing connects; The sealing that is provided with flexible material in the said sprue gate is stifled; Be provided with a mounting hole at the top of two cylindrical shell joints; The cavity volume of said mounting hole and said housing connects, be fitted with in the said mounting hole one have a volume markings glass tube, be provided with the sealing ring of flexible material between said mounting hole and the said glass tube.
Wherein, the shape of said cylindrical shell is identical, and its inside surface is the frustum surface of revolution, and two cylindrical shells are the butt end with the stub end, and the cavity volume of the formed housing in butt joint back is middle thick, the thin dolioform cavity volume in two.Said mounting hole is by laying respectively at the circular hole that two semicircle vertical slot obvolvents on the butt joint cylindrical shell surface of contact form.
The method of testing of utilizing above-mentioned Hirschfeld-Klinger reaction shrinkage factor proving installation to carry out the Hirschfeld-Klinger reaction shrinkage factor may further comprise the steps:
Step 1, if adopt above-mentioned before a kind of Hirschfeld-Klinger reaction shrinkage factor proving installation of structure, then on the inwall of said cylindrical shell, apply release agent, cast lid and capping are connected to hermetically the two ends of said cylindrical shell; If adopt the Hirschfeld-Klinger reaction shrinkage factor proving installation of above-mentioned back a kind of structure, then on the inwall of said cylindrical shell, apply release agent, with two cylindrical shell butt joints firmly, two cast lids are connected to the two ends to two cylindrical shells that connect respectively hermetically;
Step 2, sealing ring is put into the glass tube that will have volume markings behind the mounting hole more closely be inserted in the sealing ring;
Step 3, just curable if fluid to be measured need add adjuvant then mixes in proportion fluid to be measured and adjuvant; If fluid to be measured can solidify voluntarily, then liquid is got ready and got final product;
Step 4, the potpourri of fluid to be measured or fluid to be measured and adjuvant is injected cavity lentamente through the sprue gate, the root of sight glass pipe, when the liquid level in the cavity reached 0 groove of glass tube, it was stifled to seal up sealing;
Step 5, in glass tube, inject a kind of memorize liquid as label layer; This memorize liquid be a kind of neither with cavity in fluid to be measured or fluid to be measured and adjuvant potpourri generation Hirschfeld-Klinger reaction and the curing of the potpourri of fluid to be measured or fluid to be measured and adjuvant had no influence; Meanwhile, this memorize liquid is non-volatile liquid; This memorize liquid filling is arrived till the centre position of its liquid level arrival glass tube;
The potpourri of step 6, fluid to be measured or fluid to be measured and adjuvant begins in the chamber, slowly to solidify, and in solidification process, observes and write down the scale value of label layer liquid level in the glass tube, till registration no longer changes;
In above-mentioned solidification process: obtaining the shrinkage factor that the potpourri of fluid to be measured or fluid to be measured and adjuvant solidifies is:
Wherein: δ---shrinkage factor; V
0---the volume of housing; Δ v---volume change;
Step 7, according to each shrinkage factor constantly in the potpourri process of setting of the above-mentioned fluid to be measured that obtains or fluid to be measured and adjuvant, that draws fluid to be measured or fluid to be measured and adjuvant mixes the time dependent curve of its shrinkage factor.
Compared with prior art, the beneficial effect of Hirschfeld-Klinger reaction shrinkage factor proving installation of the present invention and method of testing thereof is:
Because the inner chamber of Hirschfeld-Klinger reaction shrinkage factor proving installation middle shell of the present invention is a taper type, convenient dismounting of solidifying the back sample object.Once curing is completed, sample skids off from the end of the big end one of taper type naturally.In addition, the sprue gate is arranged on the little head end that is positioned at the taper type inner chamber on the housing, holds cast by the microcephaly, bubble can be discharged from the glass tube that is bonded in the bigger end of taper type inner chamber area swimmingly.
The glass tube that has volume markings is a volume change record pipe; This glass tube is connected through a self-adapting seal ring with housing, and this self-adapting seal ring can adopt fluid sealant to make usually, and it can be regulated according to the volume change of sealing part voluntarily; Can play effect fixing and protection to glass tube; The external diameter of sealing ring guarantees good seal than the diameter of the mounting hole on the housing slightly more greatly, thereby guarantees the strict leakproofness of housing.The glass tube that has volume markings is the fluid identification layer that certain altitude is housed in the volume change record pipe, can read the volume change Δ v that solidifies sample through the fluid identification layer.Obtain the variation of volume in the measured material process of setting through the variation of fluid identification layer in the volume change record glass tube, directly read the variable quantity of volume, its test is more convenient, more accurate.And the overall process that can follow the tracks of curing.
Description of drawings
Fig. 1 is a Hirschfeld-Klinger reaction shrinkage factor proving installation single cylinder structure cut-open view of the present invention;
Fig. 2 is a Hirschfeld-Klinger reaction shrinkage factor proving installation binocular structure cut-open view of the present invention;
Fig. 3 is the structural representation of the cylindrical shell of taper type shown in Fig. 11;
Fig. 4 is that 2 structural representation is covered in cast shown in Fig. 1;
Fig. 5 is the structural representation of capping shown in Fig. 13;
Fig. 6 utilizes proving installation of the present invention to record the time dependent curve of a sample shrinkage factor;
Fig. 7 utilizes proving installation of the present invention to record the time dependent curve of another sample shrinkage factor.
Among the figure:
1---cylindrical shell 2---cast covers 3---capping
41---taper type cavity volume 42---dolioform cavity volume 5---sprue gates
6---stifled 7---sealing ring 8---glass tubes of sealing
9---mounting hole 91---first semicircle vertical slot 92---the second half garden vertical slots
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done to describe in further detail.
Fig. 1 shows a kind of structure of Hirschfeld-Klinger reaction shrinkage factor proving installation of the present invention; Comprise housing; Said housing is made up of with capping 3 cylindrical shell 1 and the cast lid 2 that is connected in said cylindrical shell 1 two ends respectively; As shown in Figure 3, the cavity volume of said housing is a taper type cavity volume 41, and said cast lid 2 is positioned at the little head end of said taper type cavity volume 41.As shown in Figure 4; The top of said cast lid 2 is provided with the sprue gate 5 that the cavity volume with said housing connects; The passage at this sprue gate 5 is one to cover the cavity volume that leads to of 2 axis tilts with cast, why sprue gate 5 is designed to inclined hole, be for the liquid that makes injection be slowly to flow in the cavity volume along the inclined hole wall; Too much air can be brought into when avoiding straight hole to inject, test result can be influenced thus.In order to process the through hole of this inclination, cast cover 2 tip designs for the tapered plane of the axis normal of this inclined via-hole, the inclined design one that 2 tops are covered in said cast is for the convenience of punching, the one, during cavity volume, liquid can flow out along the inclined-plane when liquid is filled with.It is stifled 6 to be provided with the sealing of flexible material in the said sprue gate 5, and it is also identical with the inclined hole gradient that the end of 2 sealing stifled 6 cover in cast, guarantees that sealing stifled 6 covers 2 medial surface at grade with pouring into a mould, thereby accurately guarantees the volume of cavity volume.On the oblique section of cast tops, be provided with threaded hole, the one, play the role of positioning, the one, be used for sealing stifled 6 is sealed with cavity, can sealing be blocked up 6 when preventing the volumetric expansion of material in the solidification process because the chamber eject.
Be provided with a mounting hole 9 in said cylindrical shell 1 and the junction that said capping 3 is positioned at the top, i.e. the installation position set of glass tube 8 is positioned at the top of the major part of said taper type cavity volume 41.Because, can produce bubble in cast in cavity volume during liquid, gas can be discharged at highest point smoothly, and therefore, it also is the discharge that helps bubble that glass tube is installed in the mounting hole of highest point.Said mounting hole 9 is circular holes that formed by second semicircle vertical slot 92 (as shown in Figure 3) obvolvent on first semicircle vertical slot 91 (as shown in Figure 5) on said capping 3 end faces and said cylindrical shell 1 end face; This can guarantee further that this hole is positioned at the peak of cavity volume; Utilize bubble to discharge at peak; Said mounting hole 9 connects with the cavity volume of said housing; Be fitted with in the said mounting hole 9 one have a volume markings glass tube 8, the bottom of the said first semicircle vertical slot 91 is a platform, the most the location height of glass tube 8.Be provided with the sealing ring 7 of flexible material between said mounting hole 9 and the said glass tube 8.Sealing ring 7 adopt can conformal self-adaptation adjustment shape soft gate material; For example: can adopt fluid sealant to make; It can be regulated according to the volume change of sealing part voluntarily adaptively, can play effect fixing and protection to glass tube 8, and the external diameter of sealing ring 7 than the diameter of the mounting hole on the housing 5 slightly more greatly; Guarantee good seal, thereby guarantee the strict leakproofness of housing.
In order to improve the computational accuracy of test; Can adopt the structure of double shell butt joint; As shown in Figure 2, the Hirschfeld-Klinger reaction shrinkage factor proving installation of this structure comprises housing, and axially cylindrical shells 1, two cast lids 2 that are fixed on the cylindrical shell two ends after the butt joint respectively of butt joint constitute said housing by two; The shape of said cylindrical shell 1 is identical, and its inside surface is the frustum surface of revolution, and two cylindrical shells are the butt end with the stub end, and the cavity volume of the formed housing in butt joint back is middle thick, the thin dolioform cavity volume 42 in two.The top of said cast lid 2 is provided with the sprue gate 5 that the cavity volume with said housing connects; Be provided with the sealing stifled 6 of flexible material in the said sprue gate 5; Be provided with a mounting hole 9 at the top of two cylindrical shell 1 joints; Said mounting hole 9 is by laying respectively at the circular hole that two semicircle vertical slot 92 (as shown in Figure 3) obvolvents on the butt joint cylindrical shell surface of contact form, thereby can guarantee that this circular hole is the peak of cavity volume, is beneficial to the discharge of bubble; Otherwise, if bubble does not have emptying, then can occupy the volume of measured material, so that volume is unreal, test inaccurate.Said mounting hole 9 connects with the cavity volume of said housing, be fitted with in the said mounting hole 9 one have a volume markings glass tube 8, be provided with the sealing ring 7 of flexible material between said mounting hole 9 and the said glass tube 8.
Being connected of middle cylinder body of the present invention and two end cap can adopt bolt to connect, and on the surface of contact of cylindrical shell and two end cap, will apply fluid sealant, to guarantee the airtight of cavity volume.
Utilizing Hirschfeld-Klinger reaction shrinkage factor proving installation of the present invention to carry out the test of Hirschfeld-Klinger reaction shrinkage factor may further comprise the steps:
Step 1, if adopt the Hirschfeld-Klinger reaction shrinkage factor proving installation of above-mentioned monotubular structure, then on the inwall of said cylindrical shell 1, apply release agent, with cast cover 2 and capping 3 be connected to the two ends of said cylindrical shell 1 hermetically; If adopt the Hirschfeld-Klinger reaction shrinkage factor proving installation of above-mentioned bitubular docking structure, then on the inwall of said cylindrical shell 1, apply release agent, with two cylindrical shells butt joints firmly, 2 two ends that are connected to hermetically respectively two cylindrical shells that connect are covered in two cast;
Step 2, sealing ring 7 is put into the glass tube 8 that will have volume markings behind the mounting holes 9 more closely be inserted in the sealing ring 7;
Step 3, just curable if fluid to be measured need add adjuvant; Then fluid to be measured and adjuvant are mixed in proportion, its adjuvant can be selected from a kind of thermoplastic resins such as polyvinyl acetate (PVA), polymethylmethacrylate and polystyrene, or a kind of unsaturated polyester resin all can; If fluid to be measured can solidify voluntarily; Like thermoset resin, epoxy glue etc., then liquid is got ready and to be got final product;
Step 4, the potpourri of fluid to be measured or fluid to be measured and adjuvant is injected cavity lentamente through sprue gate 5, the root of sight glass pipe when the liquid level in the cavity reaches 0 groove of glass tube, is sealed up sealing stifled 6;
Step 5, in glass tube 8, inject a kind of memorize liquid as label layer; This memorize liquid be a kind of neither with cavity in fluid to be measured or fluid to be measured and adjuvant potpourri generation Hirschfeld-Klinger reaction and the curing of the potpourri of fluid to be measured or fluid to be measured and adjuvant had no influence; Meanwhile, this memorize liquid is non-volatile liquid; This memorize liquid filling is arrived till the centre position of its liquid level arrival glass tube;
The potpourri of step 6, fluid to be measured or fluid to be measured and adjuvant begins in the chamber, slowly to solidify, and in solidification process, observes and write down the scale value of label layer liquid level in the glass tube, till registration no longer changes;
In above-mentioned solidification process: obtaining the shrinkage factor that the potpourri of fluid to be measured or fluid to be measured and adjuvant solidifies is:
Wherein: δ---shrinkage factor; V
0---the volume of housing; Δ v---volume change;
Step 7, according to each shrinkage factor constantly in the potpourri process of setting of the above-mentioned fluid to be measured that obtains or fluid to be measured and adjuvant, that draws fluid to be measured or fluid to be measured and adjuvant mixes the time dependent curve of its shrinkage factor.
In addition, in above-mentioned test process, (as: unsaturated polyester resin is under some proportionings of thermoplastic resin and adjuvant, for another example: epoxy glue) can adopt hot-water soak to improve fluid ability for the material of, thickness poor for normal temperature current downflow property.And more violent exothermic heat of reaction can take place in some prescription (as: unsaturated polyester resin, thermoplastic resin is under some proportionings of epoxy resin and adjuvant and ultraviolet light (UV) curing adhesive), can adopt water-cooled method.
Be example with the test epoxy coating below, further stress in above-mentioned test process, should note down several aspect:
(1) release agent must be smeared evenly and, can from cavity volume, take out smoothly with the convenient epoxy coating that solidifies comprehensively.
(2) want strict seal, otherwise because the poorly sealed close leakage that causes epoxy coating, cavity volume is in communication with the outside, and it will be no longer accurate causing recording volumetric shrinkage.
Epoxy coating will fully stir during (3) with epoxy coating and hardening agent, make epoxy coating is evenly mixed with hardening agent, so that can evenly solidify.
When (4) potpourri of epoxy coating and hardening agent being injected cavity volume, must be slow, let bubble discharge smoothly, otherwise when solidifying because the existence of bubble will influence the accurate measurement of volume.
(5) epoxy coating is in solidification process, and the violent therefore time interval of record of volume change at the beginning should lack, and at the after-stage that solidifies, volume change is slow, and the time interval of record can suitably be grown.
Be measured as its beneficial effect of example explanation with the volumetric shrinkage of epoxy coating.
The epoxy coating of two kinds of different proportionings is tested respectively, and the shrinkage factor of noting two samples and calculates total shrinkage factor over time.Fig. 6 utilizes proving installation of the present invention to record the time dependent curve of a sample shrinkage factor; Fig. 7 utilizes proving installation of the present invention to record the time dependent curve of another sample shrinkage factor; Change curve by record can be seen different response characteristics, and promptly volume change is inequality in the process of solidifying.It is very fast that Fig. 6 shows a sample curing rate; The chemical reaction heating is also fast, causes temperature to rise, so material is the variation of expanding within preceding 10~20 minutes after the cast; After this begin rapid contraction, about 100 minutes after the cast, reach more than 80% of total shrinkage.4 hours post-shrinkage ratios in cast basically no longer change.It is slower that Fig. 7 shows another sample curing rate, and the chemical reaction heating is also slow, and temperature variation is not obvious, so after cast, be contraction change always, about 30 hours after the cast, reaches more than 80% of total shrinkage.2-3 days post-shrinkage ratios in cast basically no longer change.To sum up, utilize the volume change that the present invention can the tracking and measuring resin curing process, and then calculate the shrinkage factor of epoxy coating in solidification process, guidance is provided to production practices.
Although invention has been described for top combination figure; But the present invention is not limited to above-mentioned embodiment, and above-mentioned embodiment only is schematically, rather than restrictive; Those of ordinary skill in the art is under enlightenment of the present invention; Under the situation that does not break away from aim of the present invention, can also make a lot of distortion, these all belong within the protection of the present invention.